环氧改性硅油的合成工艺优化及其对PAN原丝预氧化过程的影响  

Optimization of the synthesis process of epoxy-modified silicone oil and its effect on the pre-oxidation process of PAN fiber

作　　者：刘福杰 刘福燕 陈鑫宏 Liu Fujie;Liu Fuyan;Chen Xinhong(Zhenjiang College,Zhenjiang 212028;School of Chemical Engineering and Materials,Changzhou Institute of Technology,Changzhou 213032;Jiangsu Alpha Purification Equipment Manufacturing Co.,Ltd.,Taizhou 214500)

机构地区：[1]镇江高等专科学校,镇江212028 [2]常州工学院化工与材料学院,常州213032 [3]江苏阿尔法净化设备制造有限公司,泰州214500

出　　处：《化工新型材料》2023年第1期113-117,共5页New Chemical Materials

基　　金：镇江市高等专科学校青年专项课题(GZQNZX2019016)。

摘　　要：以八甲基环四硅氧烷(单体)和3-缩水甘油丙基甲基硅烷(偶联剂)为原料,以1,3-双(3-缩水甘油氧丙基)-1,1,3,3-四甲基二硅氧烷为封端剂,以四甲基氢氧化铵为催化剂,通过本体聚合法合成环氧改性硅油。通过单因素方法确定了环氧改性硅油的最佳合成工艺条件:单体与偶联剂的摩尔比2∶3、催化剂用量0.1%(wt,质量分数,下同)、封端剂用量0.5%、反应温度70℃、反应时间4h,所得产物的环氧值为0.2529mol/100g,黏度为375mPa·s。FT-IR谱图中,910cm^(-1)和3047cm^(-1)处吸收峰归属于产物中的环氧基团;热重分析表明,该环氧改性硅油具有较好的热稳定性。当环氧改性硅油乳液的附着量为1%时,可显著抑制聚丙烯腈(PAN)原丝预氧化过程中出现的粘连问题。Using octamethyl cyclotetrasiloxane(monomer) and 3-glycidyloxypropyl methylsilane(coupling agent) as raw materials, 1,3-bis(3-glycidoxypropyl)-1,1,3,3-tetramethyldisiloxane as a blocking agent and tetramethylammonium hydroxide as a catalyst, an epoxy-modified silicone oil was synthesized by bulk polymerization method.A single factor method was used to determine the optimal synthesis process conditions of epoxy-modified silicone oil, which corresponded to the molar ratio of monomer to coupling agent of 2∶3,the amount of catalyst of 0.1wt%,and the capping agent dosage of 0.5wt% at 70℃ for 4h.Under this condition, the epoxy value and viscosity of the as-synthesized epoxy-modified silicone oil was 0.2529mol/100g and 375mPa·s respectively.The absorption peaks at 910cm^(-1)and 3047cm^(-1)in the infrared spectrum were attributed to the epoxy group of the as-synthesized silicone oil.Thermogravimetric analysis showed that the as-synthesized epoxy-modified silicone oil had good thermal stability.When the adhesion amount of as-synthesized epoxy-modified silicone oil emulsion was 1wt%,the adhesion problem during the pre-oxidation of PAN could be significantly suppressed.

关 键 词：环氧改性硅油 聚丙烯腈 预氧化 本体聚合 

分 类 号：O613[理学—无机化学] TQ342[理学—化学]